1,5-Dibromopentane → HCID 54472139, 화합물

HRID 329257노트

반응식

HRID 329257 반응식
[H-].[K+].O1CCOCC1.[CH:9]([S:12][CH2:13][S:14](=[O:18])[CH:15]([CH3:17])[CH3:16])([CH3:11])[CH3:10].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]Br>C(Cl)Cl>[CH:9]([S:12][C:13]1([S:14](=[O:18])[CH:15]([CH3:17])[CH3:16])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1)([CH3:11])[CH3:10]

참가 물질

6

반응물 4

HCID 81001,5-DibromopentaneHCID 312751,4-DioxaneHCID 82127Potassium hydrideHCID 12426219HCID 12426219, 화합물

생성물 1

HCID 54472139HCID 54472139, 화합물수율 59%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Potassium hydride (995 mg) was suspended in 15 ml. of dioxane, and with ice cooling, 1.804 g of formaldehyde diisopropyl mercaptal S-oxide was added gradually. The mixture was stirred for 1 hour with ice cooling, and then 2.411 g of 1,5-dibromopentane was added. Then, the mixture was stirred for 18 hours at room temperature. Methylene chloride (100ml) was added, and the isoluble matter was separated by filtration. After the evaporation of the filtrate at reduced pressure, the residue was separated by column chromatography (basic alumina, eluted with benzene, methylene chloride, and ethyl acetate) to afford 1.463 g of cyclohexanone diisopropyl mercaptal S-oxide as a colorless oil. The yield was 59%. The physical properties and the results of elemental analysis were as follows:

후처리

  1. stirringThen, the mixture was stirred for 18 hours at room temperature
  2. customthe isoluble matter was separated by filtration
  3. customAfter the evaporation of the filtrate at reduced pressure
  4. customthe residue was separated by column chromatography (basic alumina, eluted with benzene, methylene chloride, and ethyl acetate)

출처 및 근거

ORD 기록
ord-ac3f66267eb94e6b8dd673b63e31d3f2
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04020171

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